CN102531591A - Dielectric composition having high dielectric constant, multi layered ceramic condensers comprising the same, and method of preparing for multi layered ceramic condensers - Google Patents

Dielectric composition having high dielectric constant, multi layered ceramic condensers comprising the same, and method of preparing for multi layered ceramic condensers Download PDF

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Publication number
CN102531591A
CN102531591A CN2011103501662A CN201110350166A CN102531591A CN 102531591 A CN102531591 A CN 102531591A CN 2011103501662 A CN2011103501662 A CN 2011103501662A CN 201110350166 A CN201110350166 A CN 201110350166A CN 102531591 A CN102531591 A CN 102531591A
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accessory constituent
dielectric combination
dielectric
mole
under
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Inventor
姜晟馨
宋旻星
崔斗源
权祥勋
金昶勋
许康宪
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Samsung Electro Mechanics Co Ltd
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Samsung Electro Mechanics Co Ltd
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Priority claimed from KR1020110081718A external-priority patent/KR20120089549A/en
Application filed by Samsung Electro Mechanics Co Ltd filed Critical Samsung Electro Mechanics Co Ltd
Publication of CN102531591A publication Critical patent/CN102531591A/en
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    • C04B2235/6582—Hydrogen containing atmosphere

Abstract

A dielectric composition having a high dielectric constant, multi layered ceramic condensers comprising the same, and a method of preparing for multi layered ceramic condensers. The dielectric composition includes: a compound represented by general formula (Ba1-XCax)m(Ti1-yZry)O3 (0.995<=m<=1.010, 0.001<=x<=0.10, 0.001, 0.001<=y<=0.20) as a main component; an Al oxide as a first sub-component; at least one metal selected from a group consisting of Mg, Sr, Ba, Ca, and Zr and the salt thereof, as a second sub-component; at least one metal selected from a group consisting of Sc, Y, La, Ac, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu and the salt thereof, as a third sub-component; at least one metal selected from a group consisting of Cr, Mo, W, Mn, Fe, Co, and Ni and the salt thereof, as a fourth sub-component; and a fifth sub-component selected from Si containing glass forming compounds.

Description

Have high-k dielectric combination, comprise the preparation method of its laminated ceramic capacitor and laminated ceramic capacitor
Quoting of related application
The application require in being entitled as of submitting to of on November 8th, 2010 and on August 17th, 2011 " Dielectric Composition Having High Dielectric Constant; Multi LayeredCeramic Condensers Comprising the Same; and Method of Preparing for MultiLayered Ceramic Condensers (have high-k dielectric combination, comprise the preparation method of its laminated ceramic capacitor and laminated ceramic capacitor) " korean patent application series number 10-2010-0110368 and the rights and interests of 10-2011-0081718, thus its full content is incorporated among the application by reference.
Technical field
The present invention relates to a kind of dielectric combination (dielectric composition with high-k; Dielectric composition), comprise its laminated ceramic capacitor and be used for the preparation method of laminated ceramic capacitor; More specifically, relate to a kind of dielectric combination with Y5V characteristic that satisfying of high-k define in the EIA standard, comprise its MLCC and be used for the preparation method of laminated ceramic capacitor.
Background technology
Be molded as sheet as main ingredient and the MOX that is used for control characteristic as the ceramic dielectric material of accessory constituent based on the powder of barium titanate and prepare comprising through repeating according to the laminated ceramic capacitor of association area with the preparation raw cook (green sheet) and the technology that is layered on the raw cook that will print electrode.
In nearest electronics and electrical industry, high integrated, microminiaturized and lightly fast-developing.Therefore, there is demand for the ceramic condenser that has high capacitance (capacity) and small size and have thermotolerance, a safety etc.
Laminated ceramic capacitor according to the temperature profile coefficient (TCC) of electric capacity be divided into such as Y5V (-50 ℃ under 85 ℃ ± 15% to-82%), X5R (under-55 ℃ to 85 ℃ in ± 15%), X7R (-55 ℃ under 125 ℃ ± 15%) product.Be as thin as under 3 μ m or the littler situation in that dielectric layer is shaded, use product at present usually with X5R characteristic.
Simultaneously, though precious metal such as Pd, Ag etc. have been used as the internal electrode of laminated ceramic capacitor, use at present to have base metal such as Ni etc. cheaply.Under the situation of base metal of using such as Ni,, therefore should under reducing atmosphere, fire it because electrode is oxidized in sintering procedure as internal electrode.Yet when electrode was fired under reducing atmosphere, dielectric layer was reduced, and made to compare resistance.Therefore, the non-reducing dielectric material of having developed even under reducing atmosphere, can not being reduced.
Disclose in 20000-311828 number the laminated ceramic capacitor that utilizes the dielectric magnetic composition that proposes in Japanese Patent Laid and under DC electric field, have the aging variation of low electric capacity and the deterioration of low electric capacity.Yet the dielectric magnetic composition should be fired under 1270 ℃ or higher high temperature.In addition, when the dielectric layer that in laminated ceramic capacitor, has 3 μ m thickness is stacked as four layers, make the dielectric magnetic composition realize having 8085 or lower specific inductivity.Therefore, the dielectric magnetic composition maybe not can be realized the dielectric layer of laminated ceramic capacitor is thinned to the level of 2 μ m and has low specific inductivity.
Usually, when firing temperature is higher than 1250 ℃, shrink than dielectric layer such as the interior electrode layer of the base metal of Ni faster, thereby between two-layer, cause demixing phenomenon.In addition, because the increase of the possibility of the circuit defect that the clinkering phenomenon of internal electrode causes, and the possibility of circuit defect further increases when the attenuate dielectric layer.
That is, fire under 1250 ℃ or higher high temperature according to the dielectric combination needs of association area, i.e. intensive reduction is fired.Therefore, because, in chip, crack through regular meeting because the problem like electrode clinkering etc. that causes is fired in intensive reduction.Therefore, the compsn that need be able under low temperature and weak reductive condition, fire urgently.
Summary of the invention
An object of the present invention is to provide a kind of the satisfy Y5V that in the EIA standard, defines or the dielectric combination of X5R characteristic.
Another object of the present invention provides the laminated ceramic capacitor that comprises the dielectric combination with high-k.
Another object of the present invention provides a kind of preparation method of the laminated ceramic capacitor that can under low temperature and weakly reducing atmosphere, fire.
According to an illustrative embodiment of the invention, a kind of dielectric combination with high-k is provided, has comprised: as main ingredient by general formula (Ba 1-xCa x) m(Ti 1-yZr y) O 3The compound of (0.995≤m≤1.010,0.001≤x≤0.10,0.001≤y≤0.20) expression; Al oxide as first accessory constituent; At least a metal and the salt thereof in the group of forming by Mg, Sr, Ba, Ca and Zr that is selected from as second accessory constituent; As at least a metal and the salt thereof in the group of forming by Sc, Y, La, Ac, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu that is selected from of wanting for the third time component; At least a metal and the salt thereof in the group of forming by Cr, Mo, W, Mn, Fe, Co and Ni that is selected from as the 4th accessory constituent; And the 5th accessory constituent that is selected from the glass formation compound that contains Si.
Dielectric combination can comprise based on 100 moles of main ingredients be 0.001 to 1.0 mole first accessory constituent, 0.01 to 4.00 mole second accessory constituent, 0.01 to 3.0 mole want component, 0.01 to 1.5 mole the 4th accessory constituent and 0.3 to 3.5 mole the 5th accessory constituent for the third time.
Dielectric combination can satisfy Y5V or the X5R characteristic that in the EIA standard, defines.
According to another illustrative embodiments of the present invention, the laminated ceramic capacitor that comprises the dielectric combination with high-k is provided.
According to another illustrative embodiments of the present invention, a kind of preparation method who is used for laminated ceramic capacitor is provided, comprising: mixing comprises the raw material powder (undressed powder, coarse meal) of main ingredient and accessory constituent with the preparation dielectric combination; Molded and stack of dielectric compsn are with the preparation multi-layer ceramic chip; And the plasticising multi-layer ceramic chip, under reducing atmosphere, multi-layer ceramic chip is fired and reoxidized then.
Reducing atmosphere can be 0.01% to 1.0% H 2
Firing multi-layer ceramic chip can carry out under 1150 ℃ to 1250 ℃ temperature.
Embodiment
Hereinafter, will describe the present invention in detail.
Term as used in this specification is in order to explain embodiment rather than restriction the present invention.Only if clear and definite description on the contrary, otherwise singulative comprises plural form in this manual.Word " comprises " and variant will be interpreted as component, step, operation and/or the key element (element) that is meant component, step, operation and/or the key element (element) that comprises regulation but does not get rid of any other like " comprising " or " containing ".
The present invention relates to have high-k dielectric combination, comprise its laminated ceramic capacitor and be used for the preparation method of laminated ceramic capacitor.
Dielectric combination according to an illustrative embodiment of the invention can comprise as main ingredient by general formula (Ba 1-xCa x) m(Ti 1-yZr y) O 3The compound of (0.995≤m≤1.010,0.001≤x≤0.10,0.001≤y≤0.20) expression; Al oxide as first accessory constituent; At least a metal and the salt thereof in the group of forming by Mg, Sr, Ba, Ca and Zr that is selected from as second accessory constituent; As at least a metal and the salt thereof in the group of forming by Sc, Y, La, Ac, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu that is selected from of wanting for the third time component; At least a metal and the salt thereof in the group of forming by Cr, Mo, W, Mn, Fe, Co and Ni that is selected from as the 4th accessory constituent; And the 5th accessory constituent that is selected from the glass formation compound that contains Si.
The main ingredient of dielectric combination is according to an illustrative embodiment of the invention passed through at BaTiO 3In replace part of Ba and replace a part of Ti and form with Ca with Zr.In main ingredient of the present invention, Ca is replaced entering BaTiO 3In to form the partial oxygen room, reducing resistance is provided thus.Therefore, though not formation or (thinly) formation nucleocapsid structure rarely after firing, dielectric combination can show high insulation resistance.The amount of substituted Ca is 0.001≤x≤0.1 mole.When the x value surpassed 0.1 mole, temperature profile improved; Yet, the problem of normal temperature specific inductivity deterioration can appear.
In addition, replace a part of Ti so that transformation temperature moves to about 85 ℃, realize the Y5V characteristic thus and improve the normal temperature specific inductivity with Zr.The content of y is 0.001≤y≤0.20 mole, and when the y value surpassed 0.20 mole, the normal temperature specific inductivity increased; Yet, the problem of meeting appearance temperature deterioration in characteristics.
In addition, by (Ba 1-xCa x) m(Ti 1-yZr y) O 3In the main ingredient of expression, (the Ti based on 1 1-yZr y), (Ba 1-xCa x) preferably in the scope of 0.995≤m≤1.010.When the m value is lower than 0.995; Thereby be reduced easily in dielectric combination the firing under reducing atmosphere and be easy to become semiconductor material; And when it surpasses 1.010, the problem that firing temperature excessively raises and maybe not can realize the desired temperatures characteristic can appear.
Simultaneously, according to an illustrative embodiment of the invention dielectric combination can prepare through in main ingredient, comprising multiple accessory constituent.Particularly, dielectric combination can comprise based on 100 moles of main ingredients be 0.001 to 1.0 mole first accessory constituent, 0.01 to 4.00 mole second accessory constituent, 0.01 to 3.0 mole want component, 0.01 to 1.5 mole the 4th accessory constituent and 0.3 to 3.5 mole the 5th accessory constituent for the third time.
According to an illustrative embodiment of the invention; Can add as first accessory constituent of al oxide so that reduce the firing temperature in the dielectric combination; And, first accessory constituent is included in the dielectric combination in 0.001 to 1.0 mole scope based on 100 moles main ingredient.
When for the first time wanting components contents to be lower than 0.001 mole, dielectric combination maybe not can be fired under desired temperatures, and when its during above 1.0 moles, be difficult to realize the specific inductivity of the expectation of dielectric combination.
In addition, according to an illustrative embodiment of the invention dielectric combination can comprise at least a metal and the salt thereof in the group of being made up of Mg, Sr, Ba, Ca and Zr that is selected from as second accessory constituent.In dielectric combination, preferably comprising based on 100 moles main ingredient is 0.01 to 4.00 mole second accessory constituent.When for the second time wanting components contents to be lower than 0.01 mole or during above 4.00 moles, appearance maybe not can obtain the problem of high specific inductivity.
In addition, according to an illustrative embodiment of the invention dielectric combination can comprise as at least a metal and the salt thereof in the group of being made up of Sc, Y, La, Ac, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu that is selected from of wanting for the third time component.
Based on 100 moles main ingredient, in dielectric combination, preferably include 0.01 to 3.0 mole the component of wanting for the third time.When wanting for the third time components contents to be lower than 0.01 mole; The problem that high temperature accelerated aging (high-temperature accelerated life) can not reach the level of expectation can appear; And when it surpasses 3.0 moles, can occur that firing temperature raises and the problem of the dielectric constant values that may not obtain to expect or occur because the safety deterioration problem that the generation of second phase causes.
In addition, according to an illustrative embodiment of the invention dielectric combination can comprise at least a metal and the salt thereof in the group of being made up of Cr, Mo, W, Mn, Fe, Co and Ni that is selected from as the 4th accessory constituent.
Based on 100 moles main ingredient, in dielectric combination, preferably comprise 0.01 to 1.5 mole the 4th accessory constituent.When the content of the 4th accessory constituent is lower than 0.01 mole; The problem that the high temperature accelerated aging can not reach the level of expectation can appear; And when it surpasses 1.5 moles; C*R value decline (that is, this means that numerical value descends, feasible value deterioration) and electric capacity can occur and become big problem over time as electrical condenser.
The not special restriction of the salt of the metal that in second to the 4th accessory constituent, comprises.For example, one or more materials that are selected from the group of being made up of oxide compound, carbonate, muriate, acetate, alkoxide and nitride can be as the salt that is included in the metal in second to the 4th accessory constituent.
In addition, according to an illustrative embodiment of the invention dielectric combination can comprise and is selected from the 5th accessory constituent that the glass that contains Si forms compound.The not special restriction of the 5th accessory constituent is as long as it is can combine with other components in the glass composition to form the compound of glass.For example, contain the oxide compound of Si, the glass compound that contains Si etc. and can be used as the 5th accessory constituent.
Based on 100 moles main ingredient, in dielectric combination, preferably comprise 0.3 to 3.5 mole the 5th accessory constituent.When the content of the 5th accessory constituent is lower than 0.3 mole, the problem that firing temperature raises and fires windows narrow can occur, and when it surpassed 3.5 moles, firing temperature may reduce and fire window and broaden; Yet, maybe not can realize enough specific inductivity.
Under the situation of X5R characteristic, have 2500 or higher high-k (ε) by dielectric layer, and under the situation of Y5V characteristic, have 7000 or higher high-k (ε) according to the preparation of the dielectric combination of exemplary embodiment of the invention.
And, dielectric combination satisfy the Y5V characteristic that in the EIA standard, defines (-50 ℃ under 85 ℃ ± 15% to-82%) or X5R characteristic (under-55 ℃ to 85 ℃ in ± 15%) both.
That is, dielectric combination can be in the temperature lower than existing Y5V, and for example, at 1250 ℃ or lower, more preferably 1220 ℃ or lower and more weak reducing atmosphere (1% or lower H 2) under fire, thereby make and can solve because defective that high temperature or intensive reducing atmosphere produce such as crackle etc.
In addition, the present invention can provide the laminated ceramic capacitor that comprises by the dielectric layer of the dielectric combination preparation with high-k.
The preparation method who is used for laminated ceramic capacitor according to the present invention can comprise mix comprise main ingredient and accessory constituent raw material powder to prepare dielectric combination; Molded and stack of dielectric compsn are with the preparation multi-layer ceramic chip; And the plasticising multi-layer ceramic chip, under reducing atmosphere, multi-layer ceramic chip is fired and reoxidized then.
Utilizing dielectric combination to prepare under the situation of ceramic plate, can use common tackiness agent, solvent etc., need not to be limited to especially this.
Especially, according to an illustrative embodiment of the invention, the reducing atmosphere in the preparation laminated ceramic capacitor can be at 0.01～1.0% H 2Under the condition, it can be than the much lower condition of existing strong reductive condition.Therefore, firing under this weakly reducing atmosphere under the situation of laminated ceramic capacitor, can solve and under strongly reducing atmosphere, fire the many defect problems that produce in the laminated ceramic capacitor.
In addition, according to the preparation method who is used for laminated ceramic capacitor of the present invention, firing of multilayer tablet can be carried out under 1150 to 1250 ℃ low temperature.Firing of multilayer tablet according to association area mainly is only to carry out above under 1250 ℃ the high temperature.Therefore, defect problem like crackle etc. may appear.Yet according to an illustrative embodiment of the invention, firing temperature reduces, and makes thus and can address these problems.
Hereinafter, the reference implementation example is described in detail the present invention.Embodiments of the invention are provided so that more fully explain the present invention to those skilled in the art.Following embodiment can change and not limit the scope of the invention with many different forms.On the contrary, these embodiment are provided, so that make the disclosure of invention more thoroughly with complete and thought of the present invention fully conveyed to those skilled in the art.
Embodiment 1 to 11 and comparative example 1 to 12
Utilize zirconia ball as mixing/dispersion medium, will by as following table 1 shown in the raw material powder processed of compsn and ethanol/toluene and dispersion agent and tackiness agent mix, ball milling is 15 hours then.Thereby the slurry that uses preparation utilizes the coating machine with little scraper pattern to prepare the active molded tablet with 3 to 5 μ m and has the cover mold sheet (cover moldingsheet) of 10 to 13 μ m thickness.Internal electrode is impressed, plasticising, at reducing atmosphere (0.08% H 2) under as below table 1 under 1100 to 1300 ℃ temperature, fired 2 hours, then in the thermal treatment that is used to reoxidize under 1000 ℃ after 3 hours, 20 layers of 25 layers of range upon range of active molded tablets and range upon range of cover mold sheets (thickness of 10 to 13 μ m).
The Ni electrode is impressed and is stacked on the molded ceramic plate, and plasticising is used for unsticking mixture (de-binder) through the sheet of compression and cutting, under 1150 to 1250 ℃ temperature, fires then to obtain laminated ceramic capacitor.
Table 1
Figure BDA0000106486130000091
Figure BDA0000106486130000101
Experimental example
Utilize the LCR meter at electric capacity and the dielectric loss measured under 1kHz and the 1V under the normal temperature, and in the insulativity under measurement normal temperature after 60 seconds under the state that applies DC 250V.Electric capacity is measured in-55 ℃ to 85 ℃ scope with variation of temperature.Its result is shown in the table 2.
Table 2
Figure BDA0000106486130000111
As in table 1 and 2, recognizing, when the set of dielectrics timesharing of using according to exemplary embodiment of the invention, it can be fired under low temperature and weakly reducing atmosphere.In addition, can recognize that in the situation according to the dielectric combination of exemplary embodiment of the invention, the specific inductivity of the dielectric layer of all preparations is higher than the comparative example that uses the dielectric combination that departs from the scope of the invention.
And, according to the dielectric combination of exemplary embodiment of the invention satisfied the Y5V characteristic that in the EIA standard, defines (-50 ℃ under 85 ℃ ± 15% to-82%) and X5R characteristic (under-55 ℃ to 85 ℃ in ± 15%) both.
Set forth as top, according to an illustrative embodiment of the invention, the dielectric magnetic composition can be at 1250 ℃ or lower low temperature and weakly reducing atmosphere (1% or lower H 2) under fire, make thus can to solve because the defective like crackle etc. of strongly reducing atmosphere and high temperature generation.
Therefore, can be used for various dielectric medium products according to the dielectric magnetic composition of exemplary embodiment of the invention, for example, MLCC, piezoelectric element, chip inductor, chip varistor (chipvaristor), chip resistor etc.
Especially, have according to the dielectric magnetic composition of exemplary embodiment of the invention and satisfy the Y5V that in the EIA standard, defines or the high-k of X5R characteristic.
Though combined illustrative embodiments to illustrate and described the present invention; But it will be evident to one skilled in the art that; Under not deviating from, can change and change like situation the spirit and scope of the present invention that accompanying claims limited.

Claims (7)

1. dielectric combination with high-k comprises:
As main ingredient by general formula (Ba 1-xCa x) m(Ti 1-yZr y) O 3The compound of expression, 0.995≤m≤1.010,0.001≤x≤0.10,0.001≤y≤0.20;
Al oxide as first accessory constituent;
At least a metal and the salt thereof in the group of forming by Mg, Sr, Ba, Ca and Zr that is selected from as second accessory constituent;
As at least a metal and the salt thereof in the group of forming by Sc, Y, La, Ac, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu that is selected from of wanting for the third time component;
At least a metal and the salt thereof in the group of forming by Cr, Mo, W, Mn, Fe, Co and Ni that is selected from as the 4th accessory constituent; And
Be selected from the 5th accessory constituent that the glass that contains Si forms compound.
2. the dielectric combination with high-k according to claim 1; Wherein, to comprise the said main ingredient based on 100 moles be 0.001 to 1.0 mole said first accessory constituent, 0.01 to 4.00 mole said second accessory constituent, 0.01 to 3.0 mole said component, 0.01 to 1.5 mole said the 4th accessory constituent and 0.3 to 3.5 mole said the 5th accessory constituent wanted for the third time to said dielectric combination.
3. the dielectric combination with high-k according to claim 1, wherein, said dielectric combination satisfies Y5V or the X5R characteristic that in the EIA standard, defines.
4. laminated ceramic capacitor comprises the dielectric combination with high-k according to claim 1.
5. preparation method who is used for laminated ceramic capacitor comprises:
Mixing comprises the raw material powder of main ingredient and accessory constituent with the preparation dielectric combination;
Molded and range upon range of said dielectric combination is with the preparation multi-layer ceramic chip; And
The said multi-layer ceramic chip of plasticising fires and reoxidizes said multi-layer ceramic chip then under reducing atmosphere.
6. the preparation method who is used for laminated ceramic capacitor according to claim 5, wherein, said reducing atmosphere is 0.01% to 1.0% H 2
7. the preparation method who is used for laminated ceramic capacitor according to claim 5 wherein, carries out firing of said multi-layer ceramic chip under 1150 to 1250 ℃ temperature.
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Application publication date: 20120704